溶胶-凝胶法制备（Y_（1-x）Eu_x）_2O_3发光薄膜及其发光性能研究
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摘要
本论文综述了荧光粉的发展历史、现状、发展趋势及其现在先进的显示技术对新型荧光材料的要求。薄膜荧光材料是今后荧光材料研究的热点和发展趋势。
本文研究了以Y(NO_3)_3和Eu(NO_3)_3溶液作为起始原料，六次甲基四胺法和柠檬酸络合法制备稳定的溶胶，并分别采用测定透过率和粘度的方法来检测所制备的溶胶。在硅片上旋涂后热处理制得均匀而且致密的(Y_(1-x)Eu_x)_2O_3薄膜。
对溶胶—凝胶法制备的(Y_(1-x)Eu_x)_2O_3薄膜进行XRD、AFM、SEM及发光性能测试表明，在650℃下烧结3小时得到的(Y_(1-x)Eu_x)_2O_3薄膜的结晶完好，这比高温固相法的结晶温度降低了200℃，薄膜结构致密，无孔隙，属于立方晶系。激发和发射光谱显示，在240～260nm激发强度非常大，最大激发峰在248nm处；在254nm激发下，在612.5nm处有窄的强峰发射。对Eu~(3+)的发光机理作了分析阐述，其激发带主要是Eu~(3+)与O~(2-)之间的CTS激发，而发射光谱是Eu~(3+)的~5D_0→~7Fj(j=0、1、2、3、4)的跃迁发射。
对两种不同方法所制备的薄膜发光强度检测发现，柠檬酸络合法制备的薄膜发光强度只有六次甲基四胺法的73％。经过不同浓度的Eu~(3+)掺杂的发光性能检测表明，用溶胶—凝胶法制备Y_2O_3：Eu~(3+)时，掺杂浓度从常规高温固相法的6％提高到了8％。
The development history, actuality and new trend of phosphors ,as well as the requirement of the advanced technology in display were summarized in the paper. The film materials will be the focus and the development trend in the research field of phosphors from now on.
In this paper, transparent sols of yttrium oxide doped with various concentration of europium were prepared from inorganic precursors(yttrium nitrate and europium nitrate) with hexamethylene tramine and citric acid used as complexant respectively. Transmittance and viscosity of the sols were measured .The thin film of Y2O3:Eu were deposited by spin-coating method on silicon substrates and heated in the air at different temprature .The thin films were charactered by XRD, AFM and SEM. The results show that the films have been crystalled at 650 C for sintering 3 hours. Comparing with tranditional high-temperature synthesis, its temperature was reduced 200 C.The thin films are uniform and dense. They belong to cubic lattice.
The luminescent mechanism of Y2O3:Eu3+ was analysed. The excitation spectrum of thin films show a wide band between 240nm to 260nm with a peak at 248nm, which is attributed to transition towards the charge transfer state(CTS) due to Eu-O interaction. The emission spectrum excited by 254nm consists of lines in the red spectral area. These lines correspond to transition from the excited 5Do level to 7FJ (J=0,1,2,3,4) level of the Eu3+ ion. The most intense line at 612nm corresponds to the hypersensitive transition between the 5D0 and 7F2 level of the Eu3+ ion.
Finally, Compared with the emission intensity of the films ,the film prepared by citric acide method is 73 precent of that prepared by hexamethylene tramine method. The quenching concentration of Eu3+ increased from 6% to 8% by Sol-gel method.
本文研究了以Y(NO_3)_3和Eu(NO_3)_3溶液作为起始原料，六次甲基四胺法和柠檬酸络合法制备稳定的溶胶，并分别采用测定透过率和粘度的方法来检测所制备的溶胶。在硅片上旋涂后热处理制得均匀而且致密的(Y_(1-x)Eu_x)_2O_3薄膜。
对溶胶—凝胶法制备的(Y_(1-x)Eu_x)_2O_3薄膜进行XRD、AFM、SEM及发光性能测试表明，在650℃下烧结3小时得到的(Y_(1-x)Eu_x)_2O_3薄膜的结晶完好，这比高温固相法的结晶温度降低了200℃，薄膜结构致密，无孔隙，属于立方晶系。激发和发射光谱显示，在240～260nm激发强度非常大，最大激发峰在248nm处；在254nm激发下，在612.5nm处有窄的强峰发射。对Eu~(3+)的发光机理作了分析阐述，其激发带主要是Eu~(3+)与O~(2-)之间的CTS激发，而发射光谱是Eu~(3+)的~5D_0→~7Fj(j=0、1、2、3、4)的跃迁发射。
对两种不同方法所制备的薄膜发光强度检测发现，柠檬酸络合法制备的薄膜发光强度只有六次甲基四胺法的73％。经过不同浓度的Eu~(3+)掺杂的发光性能检测表明，用溶胶—凝胶法制备Y_2O_3：Eu~(3+)时，掺杂浓度从常规高温固相法的6％提高到了8％。
The development history, actuality and new trend of phosphors ,as well as the requirement of the advanced technology in display were summarized in the paper. The film materials will be the focus and the development trend in the research field of phosphors from now on.
In this paper, transparent sols of yttrium oxide doped with various concentration of europium were prepared from inorganic precursors(yttrium nitrate and europium nitrate) with hexamethylene tramine and citric acid used as complexant respectively. Transmittance and viscosity of the sols were measured .The thin film of Y2O3:Eu were deposited by spin-coating method on silicon substrates and heated in the air at different temprature .The thin films were charactered by XRD, AFM and SEM. The results show that the films have been crystalled at 650 C for sintering 3 hours. Comparing with tranditional high-temperature synthesis, its temperature was reduced 200 C.The thin films are uniform and dense. They belong to cubic lattice.
The luminescent mechanism of Y2O3:Eu3+ was analysed. The excitation spectrum of thin films show a wide band between 240nm to 260nm with a peak at 248nm, which is attributed to transition towards the charge transfer state(CTS) due to Eu-O interaction. The emission spectrum excited by 254nm consists of lines in the red spectral area. These lines correspond to transition from the excited 5Do level to 7FJ (J=0,1,2,3,4) level of the Eu3+ ion. The most intense line at 612nm corresponds to the hypersensitive transition between the 5D0 and 7F2 level of the Eu3+ ion.
Finally, Compared with the emission intensity of the films ,the film prepared by citric acide method is 73 precent of that prepared by hexamethylene tramine method. The quenching concentration of Eu3+ increased from 6% to 8% by Sol-gel method.
引文
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[3] 郑慕周．发光材料发展近况．液晶与显示，1996，1 1(6)：143～147
[4] 李孝良，万元考，胡军，等．节能灯用稀土三基色荧光粉的研制．稀有金属与硬质合金，1997，3：9～12
[5] 周建国，赵凤英，张秀英，等．Al_(18)B_4O_(33)：Eu，Tb三基色荧光体系的合成与光谱特征．化学通报，1999，1：28～31
[6] 洪广言，曾小青．等离子体平板显示用发光材料．功能材料，1999，30(3)：225～229
[7] Chang-Hong Kim, I1-Eok Kwon, Cheol-Hee Park. Phosphors for plasma display panels. Journal of Alloys and Compounds. 2000, 311:33～39
[8] 胡文波．彩色等离子体显示器用荧光粉．真空电子技术，1998，7：33～36
[9] 蒋立德．结构化学．长沙：中南工业大学出版社，1993．124～124
[10] 肖纪美，霍明远．中国稀土理论与应用研究．北京：高等教育出版社，1992．126～130
[11] 李德杰．大屏幕场助热电子发射平板显示．真空电子技术，2002，6：1-5
[12] 卢有祥．FED用荧光粉技术进展．光电技术，1998，39(4)：70-73
[13] 孔庆升．薄膜电子学．北京：电子工业出版社，1994．1
[14] Rao R P. Growth and characterization of Y_2O_3:Eu~(3+) phosphor films by sol-gel process. Solid State Commun. 1996, 99(6):439-443
[15] Zhang H X, Kam C H, Zhou Y, etal. Deposition and photoluminescence of sol-gel derived Tb~(3+):Zn_2SiO_4 films on SiO_2/Si. Thin Solid Films. 2000, 370 (1-2) :50-53
[16] Lin J, Saenger D U, Mennig M, et al.Sol-gel depositiom and characterization of Mn~(2+)-doped silicate phosphor films. Thin Solid Films. 2000, 360(1-2) :39-45.
[l7] Bondar V. Structure and luminescence properties of individual and multi-layer thin film systems based on oxide phosphors. Mater. Sci. Eng, B. 2000, 69-70:505-509
[18] Hirata G A, Mckittrick J. Physical properties of Y_2O_3:Eu luminescent films grown by MOCVD and laser ablation. Appl. Surf. Sci. 1997,113/114:509-514
[19] Cho K G, Kumar D. Luminescence behavior of pulsed deposited Eu~(3+):Y_2O_3 thin film phosphors on sapphire substrates. Appl. Phys. Lett. 1998,73(21):3058-3060
[20] Esparza A. Garcia M. Falcony C. Structural and photoluminescent characteristics of yttrium-aluminum oxide films doped with Tb, Eu or Ce. Thin Solid Films, 1998,325:14-18
[21] 刘行仁．CRT，VFD及FED显示器用的荧光粉的进展．液晶与显示，1996，3：61～64
[22] 符连社，张洪杰，邵华，等．溶胶-凝胶法稀土光学材料研究进展．稀土，1992，19(2)：49～53
[23] Tang W. Cameron D C. Electroluminescent zinc sulphide devices produced by sol-gel processing. Thin Solid Film. 1996,280:221-226
[24] Lifshitz E. Dag I. Optical properties of CdSe namoparticle films prepared by chemical deposition and sol-gel methods. Chem. Phys. Lett. 1998,288:188-196
[25] Golego N, Studenikin S A, Cocivera M. Thin film BaMgAl_(10)O_(17):Eu phosphor prepared by spray pyrolysis, J. Electrochem. Soc. 2000,147(5):1993-1996
[26] Esparza A, Garcia M, Falcony C. Structural and photoluminescent characteristic of yttrium-aluminum oxide films doped with Tb, Eu or Ce. Thin Solid Films, 1998,325(1-2):14-18
[27] Miyata T, Nakatani T. Manganese activated gallium oxide electroluminescent phosphor thin films prepared using various deposition methods. Thin Solid Film, 2000,373(1-2):145-149
[28] Inoue R, Kitagawa M, Horii Y. Luminescent mechanism of Mn emission in ZnxMgl-Xs:Mn thin films. J. Lumin. 2000,87-89(1-4):1264-1266
[29] Lee S T, Kitagawa M, Ichino K. Correlation between photoluminescent and crystal ographic characteristics in Zn_xSr_1_xS:Ce thin
films composition dependence. Appl. Surf. Sci. 1997,113-114:499-503
[30] 林军，庞茂林，韩银花，等．溶胶-凝胶工艺制备发光薄膜研究进展．无机化学学报，2001，17(2)：153-160．
[31] 逄茂林，林君，于敏等．发光薄膜的制备及应用．液晶与显示，2002，17(5)：372—377
[32] Mastio E A, Cranton W M, Thomas C B, et al. Pulsed KrF laser annealing of RF sputtered ZnS:Mn thin films. Appl. Surf. Sci. 1999,138-139:35-39
[33] Zhao X, Komuro S, Isshiki H, et al. Fabrication and optical transition dynamics of Er-doped ZnO thin films formed on Si substrates. J. Lumin. 2000,87-89(1-4):1254-1256
[34] 刘传珍，杨柏梁，李牧菊等．激光退火法制备多晶硅薄膜的研究．液晶与显示，2000，15(1)：46-52
[35] 田军，申五福，刘行仁．Eu~(2+)和Mn~(2+)激活的碱土金属铝酸盐的阴极射线发光．稀土，1990，11(5)：1～4
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